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Preparation method of polyurethane hollow microspheres

A technology of polyurethane and polyurethane prepolymer, which is applied in the field of preparation of polyurethane hollow microspheres, can solve the problems of difficult to synthesize polyurethane hollow microsphere materials, etc., and achieve the effects of excellent covering performance, excellent pressure resistance and low density

Inactive Publication Date: 2018-11-13
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the technical problem that the existing polyurethane materials are difficult to synthesize polyurethane hollow microspheres in one step, the present invention aims to provide a preparation method of polyurethane hollow microspheres

Method used

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  • Preparation method of polyurethane hollow microspheres
  • Preparation method of polyurethane hollow microspheres
  • Preparation method of polyurethane hollow microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Weigh 30g of polyhexamethylene adipate diol, vacuum-dry and dehydrate at 110°C for 2.5 hours, drop the temperature to 50°C and put it into the reaction container, then add 15g of toluene diisocyanate, 0.02g of stannous octoate catalyst and 1.9g chain extender 1,4-butanediol, control the temperature at 85°C for 2 hours, measure the amount of remaining isocyanate by di-n-butylamine method, when the remaining content of -NCO group reaches 92-98% of the theoretical remaining amount , the reaction can be stopped by heating to obtain a polyurethane prepolymer.

[0037] 2. Weigh 35g of the above-prepared polyurethane prepolymer and 30g of isooctane and mix evenly, add 100ml mass concentration of 1.0% sodium lauryl sulfate aqueous solution to stir and mix, and then use a homogeneous emulsifier under an ice-water bath to Homogeneously emulsify at 16000rpm for 5min to obtain a stable fine emulsion.

[0038] 3. Add the prepared mini-emulsion to a three-necked flask equipped wi...

Embodiment 2

[0041] 1. Weigh 30g of polyhexamethylene adipate diol, vacuum-dry and dehydrate at 110°C for 2.5 hours, drop the temperature to 50°C and put it into the reaction container, then add 15g of diphenylmethane diisocyanate and 0.02g of stannous octoate Catalyst and 2.5g chain extender 1,6-hexanediol, control the temperature at 85°C for 2h, measure the remaining isocyanate amount by di-n-butylamine method, when the remaining content of -NCO group reaches 92- At 98%, the reaction can be stopped by heating to obtain a polyurethane prepolymer.

[0042] 2. Weigh 35g of the above-prepared polyurethane prepolymer and 25g of isooctane and mix them uniformly, add 100ml of mass concentration of 1.5% cetyltrimethylammonium bromide aqueous solution to stir and mix, and then use it in an ice-water bath. Emulsify homogeneously at 16,000 rpm for 5 minutes to obtain a stable fine emulsion.

[0043] 3. Add the prepared mini-emulsion to a three-necked flask equipped with a stirrer, a thermometer an...

Embodiment 3

[0046] 1. Weigh 25g of polytetramethylene ether glycol, vacuum dry and dehydrate at 110°C for 2.5h, drop the temperature to 50°C and put it into the reaction container, then add 12g of diphenylmethane diisocyanate, 0.01g of stannous octoate catalyst and 1.9g chain extender 1,4-cyclohexanediol, control the temperature at 85°C for 2 hours, measure the amount of remaining isocyanate with di-n-butylamine method, when the remaining content of -NCO reaches 92-98% of the theoretical remaining amount , the reaction can be stopped by heating to obtain a polyurethane prepolymer.

[0047] 2. Weigh 30g of the above-prepared polyurethane prepolymer and 25g of ethyl acetate and mix evenly, add 100ml mass concentration of 1.5% dodecyl dimethyl benzyl ammonium chloride aqueous solution, stir and mix, and then put it in an ice-water bath Use a homogeneous emulsifier to homogeneously emulsify at a speed of 16000 rpm for 5 minutes to obtain a stable fine emulsion.

[0048] 3. Add the prepared m...

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Abstract

The invention discloses a preparation method of polyurethane hollow microspheres. The preparation method of the polyurethane hollow microspheres comprises the following steps: synthesizing a polyurethane prepolymer at first; and then carrying out homogeneous emulsification preparation on the polyurethane prepolymer, a hydrophobic solvent and water by miniemulsion polymerization. By a miniemulsionprocess, the prepared polyurethane hollow microspheres are adjustable in size, the wall thickness is controllable, the stability is good, and the water dispersibility is excellent. The polyurethane hollow microspheres have excellent shielding property, by the hollow structure, the heat insulation property of a coating layer can be improved, and the polyurethane hollow microspheres can be used as covering pigment, an ultraviolet-resistant additive, a hand feeling modifier and the like, and can be widely applied to the industries of coatings, papermaking, leather and the like.

Description

technical field [0001] The invention belongs to the field of material technology, in particular to a preparation method of polyurethane hollow microspheres. Background technique [0002] In recent years, polyurethane has been a research hotspot in many fields. Because polyurethane has many excellent properties, such as high mechanical strength and oxidation stability, excellent oil resistance, high flexibility and resilience, it is widely used in many fields such as adhesives, coatings, elastomers, foams and fibers. Wide application prospects. Chinese patent CN1793192A discloses a method for preparing cross-linked polyurethane microspheres. Polyurethane microspheres are prepared by dispersing and polymerizing compounds containing isocyanate groups in water. Although the prepared polyurethane microspheres have good dispersibility, they have single performance and wide application fields. restricted. [0003] Hollow microspheres have a unique structure and a good shape and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/42C08G18/48C08G18/32C08G18/34C08G18/12B01J13/14
CPCB01J13/14C08G18/12C08G18/3206C08G18/3212C08G18/3215C08G18/348C08G18/4238C08G18/4854C08G18/664C08G18/6651C08G18/6674C08G18/6685C08G18/6692C08G18/3228
Inventor 张建安张康民吴庆云吴明元杨建军
Owner ANHUI UNIVERSITY
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